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Analysis of single polymer beads for solid phase combinatorial synthesis: the determination of reactive thiol and within batch polydispersity of bead loadings

Analysis of single polymer beads for solid phase combinatorial synthesis: the determination of reactive thiol and within batch polydispersity of bead loadings
Analysis of single polymer beads for solid phase combinatorial synthesis: the determination of reactive thiol and within batch polydispersity of bead loadings
Polymer beads are the starting point of many synthetic protocols, and in a number of combinatorial syntheses such studies are based on single beads. It has therefore become important that individual beads carry the same functional group activity and quality control of populations of beads requires a knowledge of the distribution of activity between the individual beads. A procedure was developed for the measurement of the thiol loading of single copolymer beads which is based on the bleaching of Michler's hydrol [4,4'-bis(dimethylamino)diphenylcarbinol (BDC-OH)]. Flow injection colorimetry permits the small volumes of solution generated from single beads to be measured with rapid turnover and with a reproducibility of ca. 2%. The solution detection limit of 0.17 mM corresponds to a bead thiol concentration of 0.33 mmol g(-1). The procedure and the variability of a bead population were demonstrated using modified styrene-divinylbenzene copolymer beads. The apparatus allowed fast, simple and accurate determinations to be carried out on the individual polymer beads. Within a single batch of thiol-modified styrene-divinylbenzene beads thiol loadings ranged from mol per bead. Polydispersity may therefore significantly influence screening decisions based on single bead syntheses.
0003-2654
538-541
Freeman, C.E.
de28641c-09b8-4893-9a61-69fcd76ac7d5
Howard, A.G.
12632e33-1266-49ec-ab18-8ca20c4dee72
Freeman, C.E.
de28641c-09b8-4893-9a61-69fcd76ac7d5
Howard, A.G.
12632e33-1266-49ec-ab18-8ca20c4dee72

Freeman, C.E. and Howard, A.G. (2001) Analysis of single polymer beads for solid phase combinatorial synthesis: the determination of reactive thiol and within batch polydispersity of bead loadings. Analyst, 126 (4), 538-541. (doi:10.1039/b007091m).

Record type: Article

Abstract

Polymer beads are the starting point of many synthetic protocols, and in a number of combinatorial syntheses such studies are based on single beads. It has therefore become important that individual beads carry the same functional group activity and quality control of populations of beads requires a knowledge of the distribution of activity between the individual beads. A procedure was developed for the measurement of the thiol loading of single copolymer beads which is based on the bleaching of Michler's hydrol [4,4'-bis(dimethylamino)diphenylcarbinol (BDC-OH)]. Flow injection colorimetry permits the small volumes of solution generated from single beads to be measured with rapid turnover and with a reproducibility of ca. 2%. The solution detection limit of 0.17 mM corresponds to a bead thiol concentration of 0.33 mmol g(-1). The procedure and the variability of a bead population were demonstrated using modified styrene-divinylbenzene copolymer beads. The apparatus allowed fast, simple and accurate determinations to be carried out on the individual polymer beads. Within a single batch of thiol-modified styrene-divinylbenzene beads thiol loadings ranged from mol per bead. Polydispersity may therefore significantly influence screening decisions based on single bead syntheses.

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Published date: 1 April 2001

Identifiers

Local EPrints ID: 19479
URI: http://eprints.soton.ac.uk/id/eprint/19479
ISSN: 0003-2654
PURE UUID: 9ff28e6c-6dd1-4eb2-b2f2-d11d0c84a3fc

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Date deposited: 16 Feb 2006
Last modified: 15 Jul 2019 19:27

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